Analysis method of Calcium Carbonate vitamin D3 Zinc Gluconate and Magnesium hydroxide suspension

1.0 OBJECTIVE
1.1 To lay down a procedure for analysis of Calcium Carbonate, Vitamin D3, Zinc Gluconate and Magnesium hydroxide Suspension.

2.0 SCOPE

2.1 This procedure is applicable to the analysis of Calcium Carbonate, vitamin D3, Zinc Gluconate and Magnesium hydroxide Suspension quality control laboratories

3.0 RESPONSIBILITY
3.1 Q.C- Chemist

4.0 ACCOUNTABILITY
4.1 Manager-Quality Assurance

5.0 PROCEDURE
5.1 Description: Pour 50ml finish sample in beaker and observed visually.
5.2 pH: Taken 50 ml sample in beaker rinse the pH electrode first with purified water followed by sample dip the electrode in sample and observed the pH.

5.3 Volume variation: Measured the volume by measuring cylinder and determine the volume variation.

5.4 Identification:
5.4.1 In the assay, the principle peak in the chromatogram obtain with the test solution correspond to the peak in the chromatogram obtained with the reference solution. by chemical method.
5.5 ASSAY:
Each 5.0 ml contains:
Calcium Carbonate IP (Oyster Shell) 625 mg.
Eq. to elemental calcium 250 mg.
Vitamin D3 I.P 200IU
Zinc Gluconate IP 2mg.
Magnesium hydroxide IP 75mg.

Estimation of Calcium Carbonate, Vitamin D3, Zinc Gluconate & Magnesium hydroxide
Method of Calcium Carbonate.
Titration:
Weight Accurately equivalent to 100mg. sample weight dissolve in 1 ml of hydrochloric acid. add 70 ml of water, cool and add 20 ml Ammonia solution. Titrate with 0.05 M Disodium edetate 1 ml of 0.05 M Disodium edetate is equivalent to 0.00507 gm of CaCO3

V= Volume (in ml) of Disodium edetate Solution consumed in titration.

N = Actual normality of Disodium edetate Solution.

AW= Average weight.

Wt. = Weight of Sample.

Method of (vitamin D3)

BY HPLC

Diluted solvent: Methanol

Mobile phase: METHANOL: ACETONITRILE
90: 10
Standard preparation: Weight accurately about 25 mg std wt. of vitamin D3 in 100 ml volumetric
Flask. Further dilution 1.0 ml to 250 ml volumetric flask with methanol.

Sample preparation: Weight accurately Equivalent to 0.1 mg of vitamin D3 and diluted to100 ml with methanol.

Chromatographic condition:

Wavelength -290nm
Flow rate – 1.0 ml /mint.
Column -c18 (150 x4.6) 5µm.
Temp – 350c
Retention time – about 5.70 mint
Injection volume – 100µl.

Method of zinc gluconate.

By titration:

Dissolve about 40 mg of Zinc gluconate, accurately weight in 100 ml of water. Add 5ml of ammonia-ammonia chloride buffer and 0.1 ml of

eriochrome blank (As indicator).To use and titrate with 0.005 M edetate disodium until the solution is deep in blue colour.

Each ml of 0.005 M edetate, disodium is equivalent to 2.278 mg of Zinc gluconate.

V= Volume (in ml) of Zinc Gluconate Solution consumed in titration.
N = Actual normality of Edetate Solution.
AW= Average weight
Wt. = Weight of Sample.

Calculation:

Method of Magnesium Hydroxide.
5 g of the sample is taken in 3ml of concentrated hydrochloride acid, dilute to 100ml with water, warmed on water bath and cooled.
To 25ml of sample Add 25 ml of Triethanolamine and 10 ml of Ammonia Ammonium Chloride Buffer solution. Titrate with 0.05 m E.D.T.A using erichrome black T indicator
Each ml of 0.05 M E.D.T.A is equivalent to 0.002916 of magnesium hydroxide.

Ammonia Ammonium chloride buffer:

6.75 gm Ammonium Chloride add 20 ml water and 57 ml of Ammonia produced to 100 ml water.

V= Volume (in ml) of E.D.T.A. Solution consumed in titration.

N = Actual normality of E.D.T.A Solution.

AW= Average weight.

Wt. = Weight of Sample.

6.0 ABBREVIATIONS

Sr. No.	Abbreviation used	Full form of abbreviation used
1.0	STP	Standard Testing Procedure
2.0	QA	Quality assurance
3.0	STD	Standard
4.0	SPL	Sample
5.0	I.P.	Indian Pharmacopeia
6.0	NM	Nano meter